Reaktion #323172

ord-f87341538a644f02b389ec24f511ea04

Lösungsmittel

Reaktionsbedingungen

Temperatur
195°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Waschenthe resulting solution is washed with water twice
  2. 2
    TrocknenThe dichloromethane solution is dried
  3. 3
    Sonstigeevaporated
  4. 4
    workup.DISTILLATIONthe residue distilled at reduced pressure
  5. 5
    SonstigeThe distillate is recrystallized from hot hexane

Vorschrift

A mixture of cyclohexyl isocyanate (50 mmoles), N-(2-chloroethyl)-2-oxazolidinone (50 mmoles) and anhydrous AlCl3 (40 mg, 0.3 mmole) is heated at 195° C. for 6 hours with stirring. The reaction mixture is dissolved in dichloromethane and the resulting solution is washed with water twice. The dichloromethane solution is dried and evaporated and the residue distilled at reduced pressure. The distillate is recrystallized from hot hexane to give a 50 percent yield of the desired product, m.p. 60° C.-64° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04642351uspto-grants-1987_02